Sulfuric Acid → HCID 178498115, 화합물

HRID 416571노트

반응식

HRID 416571 반응식
[OH:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[C:16]1(C)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:16][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[N:10][C:2]=1[OH:1]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 1140TolueneHCID 11430Potassium CarbonateHCID 178418543HCID 178418543, 화합물

생성물 1

HCID 178498115HCID 178498115, 화합물수율 84%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-hydroxynicotinic acid (3-067-01) (50 g) in methanol (500 ml) were added conc. sulfuric acid (15 ml) and toluene (100 mL) at room temperature. After the reaction mixture was stirred for 28 h attached Dienstark reflux tube and neutralized with an aqueous potassium carbonate solution, the solvent was evaporated. To the residue were added aqueous saturated ammonium chloride solution and chloroform, and the organic layer was separated, and the aqueous layer was extracted with chloroform. The combined organic layers were dried over anhydrous magnesium sulfate, and evaporated under reduced pressure to give 2-hydroxynicotinic acid methyl ester (3-067-02) (46 g, 84%) as a white solid.

후처리

  1. temperaturereflux tube
  2. customthe solvent was evaporated
  3. additionTo the residue were added aqueous saturated ammonium chloride solution and chloroform
  4. customthe organic layer was separated
  5. extractionthe aqueous layer was extracted with chloroform
  6. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-dc4e39f386264f54b331d1bb4335e178
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088924B2

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